CN107441150A - The technique of general flavone in a kind of spina gleditsiae using supercritical carbon dioxide extraction - Google Patents
The technique of general flavone in a kind of spina gleditsiae using supercritical carbon dioxide extraction Download PDFInfo
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- CN107441150A CN107441150A CN201710504260.6A CN201710504260A CN107441150A CN 107441150 A CN107441150 A CN 107441150A CN 201710504260 A CN201710504260 A CN 201710504260A CN 107441150 A CN107441150 A CN 107441150A
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- general flavone
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- spina gleditsiae
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/483—Gleditsia (locust)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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Abstract
The present invention disclose the technique of general flavone in spina gleditsiae using supercritical carbon dioxide extraction a kind of, belongs to the abstraction technique field of general flavone, including step, and 1) dry：By Chinese medicine Chinese honey locust thorn vacuum and low temperature drying；2) crush：Pulverize and sieve, add in supercritical extract tank；3) supercritical extract：It is 10 20L/h according to every 100g spina gleditsiae carbon dioxide flow, entrainer uses absolute ethyl alcohol and ethyl acetate according to volume ratio for 7:The mixed solution of 3 compositions, extraction time are 4 10h, and extraction temperature is 30 40 DEG C, and pressure is 15 25MPa；4) general flavone extract：By the extract of step 3), through rotary evaporation in vacuo residual ethanol and ethyl acetate, spina gleditsiae general flavone extract is obtained.The present invention is by by supercritical CO2Fluid extraction technology is applied to the extraction process of spina gleditsiae general flavone, has simple to operate a, no solvent residue in product, and extraction yield is high, it is nontoxic the advantages that.
Description
Technical field
The present invention relates to a kind of technique of general flavone in spina gleditsiae using supercritical carbon dioxide extraction, belong to total Huang
The abstraction technique field of ketone.
Background technology
Spina gleditsiae is the drying quil of legume Chinese honey locust, as traditional Chinese medicine, either simple or compound medicine,
It is all largely effective and extensive in clinical practice.《Pharmacopoeia of People's Republic of China》Version in 2010, which records spina gleditsiae, detumescence eliminating toxic,
Apocenosis, the effect of desinsection；For ulcer from the beginning of or purulence into not bursting；Control mange leprosy outside.Modern pharmacological research shows, spina gleditsiae master
Contain flavones, phenols, amino acid etc., there is the effect such as antibacterial, immunological regulation, anticancer.
The research both at home and abroad to spina gleditsiae is pharmacognosy identification and clinical practice at present, to active ingredient in spina gleditsiae
Separation Research is very few, and separation and extraction technology is also limited to extract by solvents general flavone, and recovery rate, purity are all not ideal enough.
During natural Chinese medicinal herb extracts active ingredients, except the recovery rate in view of active ingredient, also to take into account
Prevent the forfeiture of drug effect.At present, above-mentioned requirements can not also be met to the extractive technique of general flavone.
The content of the invention
In view of the above-mentioned problems of the prior art, the present invention, which provides one kind, uses supercritical carbon dioxide extraction soap
The technique of general flavone, simple to operate, no solvent residue in product, extraction yield are high in the thorn of angle.
To achieve these goals, it is provided by the invention a kind of using total in supercritical carbon dioxide extraction spina gleditsiae
The technique of flavones, specifically includes following steps,
1) dry：By Chinese medicine Chinese honey locust thorn vacuum and low temperature drying；
2) crush：Pulverize and sieve, add in supercritical extract tank；
3) supercritical extract：With carbon dioxide flow it is 10-20L/h according to every 100g spina gleditsiae, entrainer is using anhydrous
Ethanol and ethyl acetate are 7 according to volume ratio:The mixed solution of 3 compositions, extraction time 4-10h, extraction temperature 30-40
DEG C, pressure 15-25MPa；
4) general flavone extract：By the extract of step 3), through rotary evaporation in vacuo residual ethanol and ethyl acetate, soap is obtained
General flavone extract is pierced at angle.
As an improvement, the vacuum and low temperature drying temperature of the step 1) is 35-45 DEG C, drying time is 40-60 hours.
As an improvement, the screen cloth used in the step 2) is 60-100 mesh.
As an improvement, the supercritical extract condition of the step 3) is specifically, per 100g spina gleditsiae carbon dioxide flows
For 15L/h, extraction time 6h, extraction temperature is 37 DEG C, extracting pressure 18MPa.
As a further improvement, the technique specifically includes following steps,
1) dry：Chinese medicine Chinese honey locust is pierced and dried 48 hours at 40 DEG C in vacuum；
2) crush：80 mesh sieves are crushed, are added in supercritical extract tank；
3) supercritical extract：With carbon dioxide flow it is 15L/h according to every 100g spina gleditsiae, entrainer uses absolute ethyl alcohol
With ethyl acetate according to volume ratio be 7:The mixed solution of 3 compositions, extraction time 6h, extraction temperature are 37 DEG C, and pressure is
18MPa；
4) general flavone extract：By the extract of step 3), through rotary evaporation in vacuo residual ethanol and ethyl acetate, soap is obtained
General flavone extract is pierced at angle.
Compared with prior art, the beneficial effects of the invention are as follows：
1) present invention is by by supercritical CO2Fluid extraction technology is applied to the extraction process of spina gleditsiae general flavone, has
Simple to operate, no solvent residue in product, extraction yield is high, it is nontoxic the advantages that.
2) test by oxidation resistance, the general flavone extract obtained using present invention process, extract with traditional solvent
The spina gleditsiae general flavone extract for following the example of preparation is compared, and has obvious inoxidizability.
Embodiment
To make the object, technical solutions and advantages of the present invention of greater clarity, below by embodiment, the present invention is entered
Row is further described.However, it should be understood that the specific embodiments described herein are merely illustrative of the present invention, and do not have to
In limitation the scope of the present invention.
Unless otherwise defined, all technical terms and scientific terminology used herein are led with belonging to the technology of the present invention
The implication that the technical staff in domain is generally understood that is identical, and used term is intended merely to retouch in the description of the invention herein
State the purpose of specific embodiment, it is not intended that in the limitation present invention.
Embodiment one
The technique of general flavone, specifically includes following steps in a kind of spina gleditsiae using supercritical carbon dioxide extraction,
1) dry：Chinese medicine Chinese honey locust thorn is placed in vacuum, dried 60 hours at 35 DEG C；
2) crush：60 mesh sieves are crushed, are added in supercritical extract tank；
3) supercritical extract：With carbon dioxide flow it is 10L/h according to every 100g spina gleditsiae, entrainer uses absolute ethyl alcohol
With ethyl acetate according to volume ratio be 7:The mixed solution of 3 compositions, extraction time 4h, extraction temperature are 40 DEG C, and pressure is
15MPa；
4) general flavone extract：By the extract of step 3), through rotary evaporation in vacuo residual ethanol and ethyl acetate, soap is obtained
General flavone extract is pierced at angle.The extraction yield of general flavone is up to 80.7%.
The spina gleditsiae general flavone extract for taking the above method to prepare, it is configured to the general flavone that concentration is 0.05mg/mL and extracts
Thing prepare liquid, its oxidation resistance is determined using FRAP methods (iron ion reduces determination oxidative method).Experiment shows, made
Standby spina gleditsiae general flavone extract FRAP values (umol/L) are 7768.
Embodiment two
The technique of general flavone, specifically includes following steps in a kind of spina gleditsiae using supercritical carbon dioxide extraction,
1) dry：Chinese medicine Chinese honey locust thorn is placed in vacuum, dried 48 hours at 40 DEG C；
2) crush：80 mesh sieves are crushed, are added in supercritical extract tank；
3) supercritical extract：With carbon dioxide flow it is 15L/h according to every 100g spina gleditsiae, entrainer uses absolute ethyl alcohol
With ethyl acetate according to volume ratio be 7:The mixed solution of 3 compositions, extraction time 6h, extraction temperature are 37 DEG C, and pressure is
18MPa；
4) general flavone extract：By the extract of step 3), through rotary evaporation in vacuo residual ethanol and ethyl acetate, soap is obtained
General flavone extract is pierced at angle.General flavone extraction yield 86.2%.
The spina gleditsiae general flavone extract for taking the above method to prepare, it is configured to the general flavone extract that concentration is 0.1mg/mL
Prepare liquid, its oxidation resistance is determined using FRAP methods (iron ion reduces determination oxidative method).Experiment shows, prepared
Spina gleditsiae general flavone extract FRAP values (umol/L) be 8532.
Embodiment three
The technique of general flavone, specifically includes following steps in a kind of spina gleditsiae using supercritical carbon dioxide extraction,
1) dry：Chinese medicine Chinese honey locust thorn is placed in vacuum, dried 40 hours at 45 DEG C；
2) crush：100 mesh sieves are crushed, are added in supercritical extract tank；
3) supercritical extract：With carbon dioxide flow it is 20L/h according to every 100g spina gleditsiae, entrainer uses absolute ethyl alcohol
With ethyl acetate according to volume ratio be 7:The mixed solution of 3 compositions, extraction time 10h, extraction temperature are 30 DEG C, and pressure is
25MPa；
4) general flavone extract：By the extract of step 3), through rotary evaporation in vacuo residual ethanol and ethyl acetate, soap is obtained
General flavone extract is pierced at angle.General flavone extraction yield is up to 85.4%.
The spina gleditsiae general flavone extract for taking the above method to prepare, it is configured to the general flavone extract that concentration is 0.1mg/mL
Prepare liquid, its oxidation resistance is determined using FRAP methods (iron ion reduces determination oxidative method).Experiment shows, prepared
Spina gleditsiae general flavone extract FRAP values (umol/L) be 8245.
To sum up experiment shows：
Spina gleditsiae general flavone extract FRAP values (umol/L) prepared by the present invention are all higher than as 7500, oxidation resistance
Far above the general flavone extract of extract by solvents (FRAP values (umol/L) are 2642 after tested).
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modification, equivalent substitution or improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (5)
1. the technique of general flavone in a kind of spina gleditsiae using supercritical carbon dioxide extraction, it is characterised in that specifically include
Following steps,
1) dry：By Chinese medicine Chinese honey locust thorn vacuum and low temperature drying；
2) crush：Pulverize and sieve, add in supercritical extract tank；
3) supercritical extract：With carbon dioxide flow it is 10-20L/h according to every 100g spina gleditsiae, entrainer uses absolute ethyl alcohol
With ethyl acetate according to volume ratio be 7:The mixed solution of 3 compositions, extraction time 4-10h, extraction temperature are 30-40 DEG C, pressure
Power is 15-25MPa；
4) general flavone extract：By the extract of step 3), through rotary evaporation in vacuo residual ethanol and ethyl acetate, spina gleditsiae is obtained
General flavone extract.
2. the technique of general flavone in a kind of spina gleditsiae using supercritical carbon dioxide extraction according to claim 1,
Characterized in that, the vacuum and low temperature drying temperature of the step 1) is 35-45 DEG C, drying time is 40-60 hours.
3. the technique of general flavone in a kind of spina gleditsiae using supercritical carbon dioxide extraction according to claim 1,
Characterized in that, the screen cloth used in the step 2) is 60-100 mesh.
4. the technique of general flavone in a kind of spina gleditsiae using supercritical carbon dioxide extraction according to claim 1,
Characterized in that, the supercritical extract condition of the step 3) is specifically, with carbon dioxide flow be 15L/ per 100g spina gleditsiae
H, extraction time 6h, extraction temperature are 37 DEG C, extracting pressure 18MPa.
5. the technique of general flavone in a kind of spina gleditsiae using supercritical carbon dioxide extraction according to claim 1,
Characterized in that, following steps are specifically included,
1) dry：Chinese medicine Chinese honey locust is pierced and dried 48 hours at 40 DEG C in vacuum；
2) crush：80 mesh sieves are crushed, are added in supercritical extract tank；
3) supercritical extract：With carbon dioxide flow it is 15L/h according to every 100g spina gleditsiae, entrainer uses absolute ethyl alcohol and second
Acetoacetic ester is 7 according to volume ratio:The mixed solution of 3 compositions, extraction time 6h, extraction temperature are 37 DEG C, pressure 18MPa；
4) general flavone extract：By the extract of step 3), through rotary evaporation in vacuo residual ethanol and ethyl acetate, spina gleditsiae is obtained
General flavone extract.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101940745A (en) * | 2010-09-07 | 2011-01-12 | 哈药集团三精千鹤望奎制药有限公司 | Jinji blood stasis eliminating particles and preparation method thereof |
| CN103494915B (en) * | 2013-09-30 | 2015-06-10 | 侯俊光 | Preparation method and application of breast lump dissipating tablet |
-
2017
- 2017-06-28 CN CN201710504260.6A patent/CN107441150A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101940745A (en) * | 2010-09-07 | 2011-01-12 | 哈药集团三精千鹤望奎制药有限公司 | Jinji blood stasis eliminating particles and preparation method thereof |
| CN103494915B (en) * | 2013-09-30 | 2015-06-10 | 侯俊光 | Preparation method and application of breast lump dissipating tablet |
Non-Patent Citations (3)
| Title |
|---|
| 伍钦，等: "《化工实验原理》", 31 March 2014, 华南理工大学出版社 * |
| 罗永明: "《中药化学成分提取分离技术与方法》", 31 January 2016 * |
| 肖爽: "皂角刺总黄酮抗肿瘤有效组分的筛选及活性评价", 《中国优秀硕士学位论文医药卫生科技辑》 * |
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